CN107677712A - Method for testing electrochemical impedance spectrum of lithium ion battery - Google Patents
Method for testing electrochemical impedance spectrum of lithium ion battery Download PDFInfo
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- CN107677712A CN107677712A CN201710828191.4A CN201710828191A CN107677712A CN 107677712 A CN107677712 A CN 107677712A CN 201710828191 A CN201710828191 A CN 201710828191A CN 107677712 A CN107677712 A CN 107677712A
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- Prior art keywords
- electrochemical impedance
- electrode
- reference electrode
- impedance spectroscopy
- lithium ion
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 32
- 238000001453 impedance spectrum Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 14
- 238000012360 testing method Methods 0.000 title claims abstract description 4
- 238000000157 electrochemical-induced impedance spectroscopy Methods 0.000 claims description 54
- 238000010998 test method Methods 0.000 claims description 6
- 230000005518 electrochemistry Effects 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 239000010439 graphite Substances 0.000 description 9
- 229910002804 graphite Inorganic materials 0.000 description 9
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 8
- 229910052744 lithium Inorganic materials 0.000 description 8
- 230000008569 process Effects 0.000 description 7
- 229910052493 LiFePO4 Inorganic materials 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- ZSYNKHJUSDFTCQ-UHFFFAOYSA-N [Li].[Fe].P(O)(O)(O)=O Chemical compound [Li].[Fe].P(O)(O)(O)=O ZSYNKHJUSDFTCQ-UHFFFAOYSA-N 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a method for testing electrochemical impedance spectrum of a lithium ion battery, which comprises the following steps: putting the positive plate, the negative plate, the first reference electrode and the second reference electrode into a four-electrode system electrolytic cell; measuring an electrochemical impedance spectrum by taking the positive plate as a working electrode, the negative plate as a counter electrode and the first reference electrode as a reference electrode to obtain an electrochemical impedance spectrum 1; measuring an electrochemical impedance spectrum by using the positive plate as a working electrode, the second reference electrode as a counter electrode and the first reference electrode as a reference electrode to obtain an electrochemical impedance spectrum 2; measuring an electrochemical impedance spectrum by using the negative plate as a working electrode, the second reference electrode as a counter electrode and the first reference electrode as a reference electrode to obtain an electrochemical impedance spectrum 3; and comparing the measured electrochemical impedance spectrums 1, 2 and 3 to obtain the attribution of each part of the electrochemical impedance spectrum of the full cell. The invention can clearly explain the attribution of each part of the electrochemical impedance spectrum of the lithium ion battery full cell.
Description
Technical field
The present invention relates to field of lithium, more particularly to a kind of method of testing of lithium ion battery electrochemical impedance spectrum.
Background technology
Lithium ion battery is due to larger energy density, higher operating voltage, excellent cycle performance, memoryless
The advantages that effect, self-discharge rate are low, internal resistance is small and environmental pollution is small, in the electronic products such as mobile communications tool and electronic vapour
Extensive use on car.The electrode interface course of reaction of lithium ion battery is to the charge/discharge capacity of battery, cycle characteristics and forthright again
Energy, which waits, has material impact.Therefore the electrode interface course of reaction of research lithium ion battery is to illustrating its capacity attenuation mechanism, carrying
The high tool such as its circulation volume and high rate performance is of great significance.
Electrochemical impedance spectroscopy (EIS) is the important method for studying electrochemical interface process, in past more than 10 years, EIS quilts
It is widely used in grinding for insertion abjection process of the lithium ion in inlaid scheme such as carbon material, transition metal oxide
Study carefully.EIS can occur according to the difference of each step time constant of electrochemical reaction so as to obtain electrode in the range of different frequency
Differential responses.With EIS research lithium ions in the dependent dynamics parameter of the insertion abjection process of embedded particle, such as lithium ion
Diffusion coefficient of the diffusive migration by the resistance, electronic conductivity energy, charge-transfer resistance, lithium ion of SEI films inside particle
Deng, and these kinetic parameters and electrode polarization current potential, the relation of temperature, to understanding lithium ion in embedded electrode material granules
Embedded abjection mechanism, have in terms of the inefficacy mechanism of the conversion reaction mechanism of transition metal oxide, particularly lithium ion battery
Highly important effect.
However, EIS also has one than more serious limitation in the further application of electrochemical field：For with complexity
, the explanation of the composite impedance spectrum that the electrode reaction of multi-step is related it is also indefinite.On the one hand it is the electricity because lithium ion battery
Chemical impedance spectrum is generally made up of two kinds of elements, i.e. semicircle and oblique line, many different physical processes or complex process
Different step, there is similar feature in electrochemical impedance spectroscopy；On the other hand it is due to that time constant is close, different physics
Feature of the different step of process or a complex process in electrochemical impedance spectroscopy overlaps, and turns into a feature.
The content of the invention
Based on technical problem existing for background technology, the present invention proposes a kind of survey of lithium ion battery electrochemical impedance spectrum
Method for testing, to realize the purpose of each several part ownership for the electrochemical impedance spectroscopy for clearly explaining the full battery of lithium ion battery.
A kind of method of testing of lithium ion battery electrochemical impedance spectrum proposed by the present invention, comprises the following steps：
S1, positive plate, negative plate, the first reference electrode, the second reference electrode be fitted into four electrode system electrolytic cells；
S2, using positive plate as working electrode, negative plate be electrode, the first reference electrode are measured for reference electrode its electricity
Chemical impedance is composed, and obtains electrochemical impedance spectroscopy 1；
S3, using positive plate as working electrode, it is reference electrode to electrode, the first reference electrode that the second reference electrode, which is, survey
Its electrochemical impedance spectroscopy is measured, obtains electrochemical impedance spectroscopy 2；
S4, using negative plate as working electrode, it is reference electrode to electrode, the first reference electrode that the second reference electrode, which is, survey
Its electrochemical impedance spectroscopy is measured, obtains electrochemical impedance spectroscopy 3；
S5, the electrochemical impedance spectroscopy 1,2,3 that measures of contrast, show that the electrochemical impedance spectroscopy various pieces of full battery are returned
Category.
Preferably, in step 1, positive plate, negative plate, the first reference electrode, the second reference electrode are loaded same four
In electrode system electrolytic cell.
The present invention measures the electrochemical impedance of the full battery of lithium ion battery in same device under identical environment
Spectrum, the electrochemical impedance spectroscopy of lithium ion battery positive and negative electrode half-cell, avoid because different device, resistance caused by varying environment
Anti- spectral difference is different, improves the accuracy contrasted between different impedance spectrums；Electricity of the invention by comparing the full battery of lithium ion battery
Chemical impedance is composed, and the electrochemical impedance spectroscopy of lithium ion battery positive and negative electrode half-cell, can clearly explain the full battery of lithium ion battery
Electrochemical impedance spectroscopy each several part ownership.
Brief description of the drawings
Fig. 1 is the spectrogram of electrochemical impedance spectroscopy 1 that the present invention obtains.
Fig. 2 is the spectrogram of electrochemical impedance spectroscopy 2 that the present invention obtains.
Fig. 3 is the spectrogram of electrochemical impedance spectroscopy 3 that the present invention obtains.
Embodiment
Below, technical scheme is described in detail by specific embodiment.
Embodiment 1
A kind of method of testing of lithium ion battery electrochemical impedance spectrum, comprises the following steps：
S1, positive plate, negative plate, the first reference electrode, the second reference electrode be fitted into four electrode system electrolytic cells；
S2, using positive plate as working electrode, negative plate be electrode, the first reference electrode are measured for reference electrode its electricity
Chemical impedance is composed, and obtains electrochemical impedance spectroscopy 1；
S3, using positive plate as working electrode, it is reference electrode to electrode, the first reference electrode that the second reference electrode, which is, survey
Its electrochemical impedance spectroscopy is measured, obtains electrochemical impedance spectroscopy 2；
S4, using negative plate as working electrode, it is reference electrode to electrode, the first reference electrode that the second reference electrode, which is, survey
Its electrochemical impedance spectroscopy is measured, obtains electrochemical impedance spectroscopy 3；
S5, the electrochemical impedance spectroscopy 1,2,3 that measures of contrast, show that the electrochemical impedance spectroscopy various pieces of full battery are returned
Category.
Embodiment 2
A kind of method of testing of lithium ion battery electrochemical impedance spectrum, comprises the following steps：
S1, iron phosphate lithium positive pole piece, graphite cathode piece, the first lithium piece, the second lithium piece loaded into same four electrode system
In electrolytic cell；
S2, using iron phosphate lithium positive pole piece as working electrode, graphite cathode piece be to electrode, the first lithium piece for reference electrode,
Its electrochemical impedance spectroscopy is measured, obtains electrochemical impedance spectroscopy 1；
S3, using iron phosphate lithium positive pole piece as working electrode, it is reference electrode to electrode, the first lithium piece that the second lithium piece, which is, survey
Its electrochemical impedance spectroscopy is measured, obtains electrochemical impedance spectroscopy 2；
S4, using graphite cathode piece as working electrode, it is reference electrode to electrode, the first lithium piece that the second lithium piece, which is, measures it
Electrochemical impedance spectroscopy, obtain electrochemical impedance spectroscopy 3；
S5, the electrochemical impedance spectroscopy 1,2,3 that measures of contrast, show that the electrochemical impedance spectroscopy various pieces of full battery are returned
Category；
Wherein, the spectrogram reference picture 1,2,3 of the electrochemical impedance spectroscopy 1,2,3 obtained；From in Fig. 1, just extremely phosphoric acid
Iron lithium, negative pole for the full battery of graphite electrochemical impedance spectroscopy, by a semicircle of high frequency region, one section of circular arc of intermediate frequency zone and low
One oblique line composition in frequency area；From in Fig. 2, the electrochemical impedance spectroscopy of LiFePO4 half-cell, by the one and half of high frequency region
One oblique line of circle and low frequency range forms；From in Fig. 3, the electrochemical impedance spectroscopy of graphite half-cell, by one of high frequency region
Semicircle, a semicircle of intermediate frequency zone and the oblique line composition of low frequency range；Understand, just extremely LiFePO4, bear with reference to Fig. 1,2,3
High frequency region semicircle extremely in the electrochemical impedance spectroscopy of the full battery of graphite is made up of the high frequency region semicircle of LiFePO4 and graphite,
Its intermediate frequency zone circular arc is made up of the intermediate frequency zone semicircle of graphite, its low frequency range oblique line by LiFePO4 and graphite low frequency range oblique line group
Into.
It can be seen that by method of the invention, it is possible to measuring the electrochemical impedance spectroscopy of the full battery of lithium ion battery, lithium-ion electric
The electrochemical impedance spectroscopy of pond positive and negative electrode half-cell, by comparing the electrochemical impedance spectroscopy of the full battery of lithium ion battery, lithium-ion electric
The electrochemical impedance spectroscopy of pond positive and negative electrode half-cell, can clearly explain the full battery of lithium ion battery electrochemical impedance spectroscopy it is each
Part belongs to.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (2)
1. a kind of method of testing of lithium ion battery electrochemical impedance spectrum, it is characterised in that comprise the following steps：
S1, positive plate, negative plate, the first reference electrode, the second reference electrode be fitted into four electrode system electrolytic cells；
S2, using positive plate as working electrode, negative plate it is that its electrochemistry is measured for reference electrode to electrode, the first reference electrode
Impedance spectrum, obtain electrochemical impedance spectroscopy 1；
S3, using positive plate as working electrode, it is reference electrode to electrode, the first reference electrode that the second reference electrode, which is, measures it
Electrochemical impedance spectroscopy, obtain electrochemical impedance spectroscopy 2；
S4, using negative plate as working electrode, it is reference electrode to electrode, the first reference electrode that the second reference electrode, which is, measures it
Electrochemical impedance spectroscopy, obtain electrochemical impedance spectroscopy 3；
The electrochemical impedance spectroscopy 1,2,3 that S5, contrast measure, draw the ownership of the electrochemical impedance spectroscopy various pieces of full battery.
2. the method for testing of lithium ion battery electrochemical impedance spectrum according to claim 1, it is characterised in that, will in step 1
Positive plate, negative plate, the first reference electrode, the second reference electrode are fitted into same four electrode systems electrolytic cell.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710828191.4A CN107677712A (en) | 2017-09-14 | 2017-09-14 | Method for testing electrochemical impedance spectrum of lithium ion battery |
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| CN201710828191.4A CN107677712A (en) | 2017-09-14 | 2017-09-14 | Method for testing electrochemical impedance spectrum of lithium ion battery |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108519410A (en) * | 2018-03-15 | 2018-09-11 | 合肥国轩高科动力能源有限公司 | Method for representing concentration change of lithium ions in electrolyte in circulation process |
| CN108693407A (en) * | 2018-05-08 | 2018-10-23 | 湖北工业大学 | A kind of reference resistance of error minimum is to preferred impedance spectrum measurement method |
| CN108987659A (en) * | 2018-06-26 | 2018-12-11 | 桑顿新能源科技有限公司 | A kind of four electrode system of lithium ion soft-package battery and preparation method thereof |
| CN111051865A (en) * | 2018-07-06 | 2020-04-21 | 株式会社Lg化学 | Method for measuring specific surface area of conductive material |
| CN111766283A (en) * | 2020-06-23 | 2020-10-13 | 合肥国轩高科动力能源有限公司 | Diaphragm closed pore temperature testing method |
| WO2022257566A1 (en) * | 2021-06-09 | 2022-12-15 | 蜂巢能源科技股份有限公司 | Three-electrode cell structure and preparation method therefor, and method for testing negative electrode potential |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108519410A (en) * | 2018-03-15 | 2018-09-11 | 合肥国轩高科动力能源有限公司 | Method for representing concentration change of lithium ions in electrolyte in circulation process |
| CN108693407A (en) * | 2018-05-08 | 2018-10-23 | 湖北工业大学 | A kind of reference resistance of error minimum is to preferred impedance spectrum measurement method |
| CN108987659A (en) * | 2018-06-26 | 2018-12-11 | 桑顿新能源科技有限公司 | A kind of four electrode system of lithium ion soft-package battery and preparation method thereof |
| CN111051865A (en) * | 2018-07-06 | 2020-04-21 | 株式会社Lg化学 | Method for measuring specific surface area of conductive material |
| US11293854B2 (en) | 2018-07-06 | 2022-04-05 | Lg Chem, Ltd. | Measurement method for specific surface area of conductive material |
| CN111766283A (en) * | 2020-06-23 | 2020-10-13 | 合肥国轩高科动力能源有限公司 | Diaphragm closed pore temperature testing method |
| WO2022257566A1 (en) * | 2021-06-09 | 2022-12-15 | 蜂巢能源科技股份有限公司 | Three-electrode cell structure and preparation method therefor, and method for testing negative electrode potential |
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Application publication date: 20180209 |
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